CN103948565B - The double coated method of a kind of employing prepares lycopene microcapsule and preparation method thereof - Google Patents

The double coated method of a kind of employing prepares lycopene microcapsule and preparation method thereof Download PDF

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CN103948565B
CN103948565B CN201410210824.1A CN201410210824A CN103948565B CN 103948565 B CN103948565 B CN 103948565B CN 201410210824 A CN201410210824 A CN 201410210824A CN 103948565 B CN103948565 B CN 103948565B
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lycopene
microcapsule
coated
preparation
double coated
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CN103948565A (en
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敬思群
柴文杰
时慧
顾学健
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XINJIANG TEKANG BIOTECHNOLOGY Co Ltd
Xinjiang University
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XINJIANG TEKANG BIOTECHNOLOGY Co Ltd
Xinjiang University
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Abstract

The open one of the present invention uses double coated method to prepare lycopene microcapsule and preparation method thereof, by selecting suitably mixing wall material, research optimum emulsification condition and Drying Technology Parameter, supercritical extraction technique is used to combine with supertension isomerization treatment technology, preparing lycopene microcapsule by double coated method, secondary is coated the technique of the preparation of lycopene microcapsule and uses porous-starch consumption by 0.16%, and beta cyclodextrin consumption presses 0.16%, adsorption temp 50 DEG C, adsorption time 30 min;It is made to isolate with external environment in being enclosed in cyst membrane, with improve its to light and the stability of oxygen, expand range, effectively overcome technical bottleneck present in the application of current lycopene, the lycopene microcapsule cis-isomer ratio of preparation is 45 50%, and bioavailability is high;Embedding rate is up to 97.75%, and lycopene carrying capacity is 40.70 mg/g, has wide applicability and using value.

Description

The double coated method of a kind of employing prepares lycopene microcapsule and preparation method thereof
Technical field
The present invention relates to lycopene and extract the technical field of preparation.Specifically, the present invention relates to a kind of utilization be coated Method prepares the technical field of lycopene microcapsule.
Background technology
Lycopene (Lycopene), has another name called lycopene, is one of primary pigments in mature tomato, is also nature The one of the 600 multiple types carotene (Carotenoid) having been found that.Research in recent years shows, lycopene not only can be made For a kind of new type functional natural pigment, and preventing various diseases, cancer-resisting, raising immunologic function, pre-anti-aging etc. All many-sides, have stronger biological function effect.There are some researches show, daily intake the Fructus Lycopersici esculenti system containing 40mg lycopene Product, just be enough to significantly reduce low density lipoprotein, LDL (LDL) oxidation, reduce the ill danger of some disease such as cancer cardiovascular disease Danger.Therefore, lycopene usually has the laudatory title of " ensconcing the gold in Fructus Lycopersici esculenti ", FAO (Food and Agriculture Organization of the United Nation), food additive committee Member can and World Health Organization (WHO) all assert that it is A class nutrient, more than 50 countries and regions also as have nutrition with The food additive of color dual function, is widely used in the fields such as food, health product, medicine and cosmetics.
Lycopene is the many unsaturated hydrocarbons being made up of 11 conjugation and 2 unconjugated double bonds, is β-Radix Dauci Sativae Many conjugated double bonds of the isomers lycopene of element so that it is be very easy to occur cis-trans isomerization and oxidative degradation are stable The lycopene that property extreme difference, especially purity is the highest, owing to lacking the protection of other materials, extremely unstable, easy oxidized destruction.? In nature, lycopene exists with alltrans configuration (all-trans) mostly, and alltrans is also the most stable of one of thermodynamics Form.And in each tissue of human body, lycopene but exists with cis-isomer mostly, especially in prostate, cis Lycopene is up to 80%.Therefore ratio research finds, lycopene can by illumination, acid, purple extraradial affect generation isomerization [5], producing part cis-isomer, the most therefore its character change.
Super-high-pressure Food-processing Technology technology refers to utilize the pressure of more than 100MPa, room temperature or relatively low at a temperature of, make food The biomacromolecules such as enzyme, protein, ribonucleic acid and starch in product change activity, degeneration or gelatinizing, kill antibacterial etc. simultaneously Microorganism is to reach the process of sterilizing, and the natural taste of food, local flavor and nutritive value are not subject to or little affected one Processing method.At present, Food Science man has been proved the feasibility that HIGH PRESSURE TREATMENT uses at industrially scalable.Become food industry The most attractive process technology of the hot worked one of middle replacement, meets modern food " natural, nutrition, health, safety " Developing direction, meet consumer and advocate the needs of " natural, healthy ".China's ultra high pressure treatment food technology is in grinds in early days Studying carefully the stage, this block of superhigh pressure technique is used for sterilization or the extraction of food, and people does not directly promote Fructus Lycopersici esculenti as one The means of red pigment isomerization carry out studying, and there is not yet super high pressure food so far and sell on market, so accelerating to carry out superelevation Pressure food research, the meaning of particular importance that China is taken part in international competition.
Superhigh pressure technique meet non-thermal under the conditions of ensure the demand of food high-quality and microbial safety, high pressure can Stepless action is in whole food, not by the size of product and limiting to of geometry.Jin L finds that superhigh pressure technique is at low temperature Under the conditions of natural plant extracts and food can be carried out disinfection, natural plants will not be hydrolyzed, but organism generation shape can be induced State changes, and Woon Yong Choi etc. is under the conditions of 500MPa, to ginsenoside's ultra high pressure treatment 20min, finds that supertension can The ginsenoside of physical property hydrolysis high molecular, obtains the ginsenoside of the low-molecular-weight of more high bioactivity.According to strangling the summer Torr row principle is inferred, the direction that ultra high pressure treatment can promote the chemical reaction of material and molecular conformation to reduce towards volume is entered OK, the configuration of the cis-trans-isomer of lycopene can occur certain conversion.
Ines J. P. Colle etc. have studied the isomerization kinetic model of lycopene, finds that isomerization process is to temperature Degree has obvious dependency, too high temperature that lycopene can be made to be destroyed, and too low temperature slows down the generation of isomerization;Zhang Huan Big grade has inquired into the solvent method impact on lycopene isomerization, finds that in 6% lycopene oleo-resinous, cis-isomer accounting is high Cis-isomer accounting in 90% lycopene, but solvent method isomerization is inefficient, easily remain.Therefore, supertension is used Means, it is ensured that under cryogenic conditions, promote lycopene isomerization, have bactericidal effect simultaneously, have certain researching value.
Microcapsule (Microencapsule) is using macromolecular material that is natural or that synthesize as wall material, passes through physics A kind of active substance (core) is wrapped up to be formed by method, chemical method or physical-chemical process to be had semi permeability or seals the micro-of cyst membrane Type capsule.Microcapsule technology i.e. micro encapsulation, is a kind of solid or the skill of liquid filmogen embedding formation fine particle Art.The particle diameter of this fine particle can in the scope of millimeter, micron, even nanometer, according to size can be divided into nanoparticle or Nano capsule, microcapsule, microgranule and microsphere etc..During micro encapsulation, the material being embedded is referred to as core, the one-tenth of embedding core Membrane material is referred to as wall material.Wall material is typically to be formed by naturally occurring or synthetic macromolecular material, needs in microencapsulation processes Possess good mobility and dissolubility, promote that the parcel of core is to form more stable emulsion system.The side of micro encapsulation Method has spray drying method, Inclusion Complexes method, phase separation method and interfacial polymerization etc., and lycopene is the most novel current merit A focus in energy food composition research, and the research that China is in this respect is also in the starting stage.Owing to lycopene belongs to In fat-soluble, and easy oxidative degradation under the effect of light, heat and oxygen, greatly limit its use value, use micro-glue Capsule technology carries out capsulation process, can improve its stability and the availability in functional product thereof, promotes its physiology merit The performance of energy.This method has the biggest potential using value, and many materials, such as aromatic condiment essential oil, essence, pigment, vitamin etc. Material all can form Inclusion Complexes with wall material.At present about the research of lycopene microcapsule technology application, the most all exist Carry out, but still belong to preliminary.The micro encapsulation of lycopene is reported by more existing documents.
Nanjing University of Finance and Economics Qiu Wei fragrant [73], with lycopene oleo-resinous as core, uses soluble soybean polysaccharide spray dried Dry obtaining lycopene microcapsule product, membrane structure is compact and complete, but due to soybean polysaccharide used intermolecular combination power not With, there is rough problem in the surface of microcapsule prepared;Shihezi Univ grandson passes celebrating etc., and [74 have studied spray drying legal system The technique of standby microcapsule lycopene powder and technology, the lycopene good water solubility after micro encapsulation, good dispersion, but experiment Gained microcapsule efficiency, productivity is on the low side;Huainan associated university Jin Xue far waits [75] to use ultrasonic method to prepare lycopene beta-ring and sticks with paste Inclusion compounds, the inclusion rate of lycopene is up to 73.6%, and the lycopene of inclusion retention rate in 60d reaches 92.2%, but real Test gained lycopene inclusion rate relatively low, have part lycopene to remain in clathrate surface, cause a certain degree of waste.
Patent aspect at home, Shanghai Communications University Liu Rong is thick etc. has declared that " preparation method of lycopene microcapsule is (specially Profit application number 200710037308) ".The lycopene microcapsule obtained for pink, uniform particle diameter, smooth surface, free from extraneous odour, Good fluidity, there are good water solublity, content of lycopene high;Chen Henglei has declared the " production of a kind of lycopene microcapsule Method (number of patent application 201010004928) ".The method teaches the allotment of core, wall material solution, carries out homogenizing after mixing, The spray-dried lycopene microcapsule dissolubility obtained of emulsion after homogenizing is high, the good stability to light, heat and oxygen.This The least by being spray-dried gained microcapsule in general particle diameter a bit, through after a while, it is susceptible to adhesion adsorption, Product sensory is not in good state.Abroad, the technical patent of lycopene product the most always Israel is proprietary, later the U.S., Italy, Britain etc. all have developed the lycopene series products of multiple dosage form, but these patents are mostly the former of lycopene Patent in terms of material preparation.
As can be seen here, lycopene is carotenoid main in Fructus Lycopersici esculenti and tomato products, is also important in human diet Compound.Lycopene have as antioxidation, remove between free radical, inducing cell connecting communication, modulate tumor propagation etc. many Plant function.Being liposoluble substance yet with lycopene, in water, dissolubility is poor, and they are to oxygen, light and heat the most not Stable, this makes them there is significant limitation in production and processing and application.Additionally, there is cis-trans isomerism in lycopene Body, cis-isomer is easier to be absorbed than transisomer, and heat treated can make lycopene can become cis from trans, but Oxidation Decomposition also can occur, and present in lycopene, VE, plant sterol etc. also can destroy.Objective reality in these reality Technical problem be required for fabricating technology and solve.
Summary of the invention
Overcome lycopene dissolubility in water poor for not yet in effect in prior art, the most unstable to oxygen, light and heat, This makes them there is significant limitation in production and processing and application, and lycopene exists cis-trans-isomer, syn-isomerism Body is easier to be absorbed than transisomer, and heat treated can make lycopene can become cis from trans, but oxygen also can occur Changing and decompose, present in lycopene, VE, plant sterol etc. also can occur the realistic problem destroyed.The present invention needs the skill solved Art problem is that the defect overcoming prior art, it is desirable to provide a kind of use double coated method prepare lycopene microcapsule and Preparation method, the present invention is with lycopene microcapsule preparation technology as main research, by selecting suitably mixing wall material, Research optimum emulsification condition and Drying Technology Parameter, use supercritical extraction technique to tie mutually with supertension isomerization treatment technology Close, prepare lycopene microcapsule by double coated method so that it is isolate, to improve it to light with external environment in being enclosed in cyst membrane With the stability of oxygen, expand range, effectively overcome technical bottleneck present in the application of current lycopene, there is reality Extensive using value.
The present invention specifically provides a kind of method using double coated method to prepare lycopene microcapsule, and % is according to weight percent Than meter, comprising the following steps that of lycopene microcapsule.
(1) preparation of tomato peel: select without going mouldy tomato peel, removes impurity removing, and with clear water by the earth on skin slag, Foreign material cleaned standby seam.
(2) lycopene oleo-resinous is prepared: the tomato peel of above-mentioned preparation is used supercritical CO2Extraction, pressure 28MPa, extraction temperature are at 70-72.5 DEG C, and CO flow 2500 2600kg/h, extraction time: 120min, in these process conditions Under, available purity reaches the lycopene of more than 90%;The present invention is by supercritical CO in tomato peel26% be obtained by extraction kind Lycopene oleoresin is as raw material, it is ensured that without any chemical composition and dissolvent residual on raw material, safety non-toxic.
(3) lycopene purifying process: use lycopene oleo-resinous above-mentioned steps (2) provided by 1:10(w/v) Solid-liquid ratio be dissolved in normal hexane, after magnetic agitation 10min, place room temperature cooling, place into-18 DEG C of refrigerator cooling stand 12h Rear sucking filtration obtains crystal of lycopene body, by after this step repeatedly purification three times lycopene, purity is 41.8% after measured.
(4) supertension isomerization processes, the lycopene of preparation cis ratio: purification mistake above-mentioned steps (3) prepared Lycopene oleo-resinous, be dissolved in the normal hexane of 100/mL according to every 5mg lycopene oleo-resinous, install to polyethylene complex pocket Middle vacuum seals, and uses common extra-high tension unit, at 500Mpa, obtains cis-isomer at 50 DEG C under the conditions of supertension 10min Ratio 45.69%, content is the lycopene of 103.24mg/g, then uses high performance liquid chromatography to separate it, final To cis lycopene;Ultra high pressure treatment means are used effectively to promote lycopene to be changed into cis-structure from transconfiguration, Other effective ingredient in lycopene will not be hydrolyzed, moreover it is possible to play the effect of cold sterilization.
(5) employing is once coated the preparation of lycopene microcapsule: utilize ultrasonic emulsification and spray drying method to carry out Fructus Lycopersici esculenti The first time of red pigment is coated, with arabic gum and modified starch for wall material, and arabic gum and modified starch ratio 1:2 based on m/m, Solid content 10%, core wall than 1:1 based on m/m, tween 80 consumption 2%, at 30 DEG C, ultrasonic emulsification 15min under the conditions of 160W, Being spray-dried inlet temperature 190 DEG C, leaving air temp 80 DEG C, atomisation pressure 18MPa, microcapsule embedded efficiency, up to 85.12%, is produced Rate is 60.50%;The lycopene microcapsule mean diameter that is once coated obtained is 8.13 μm, and the particle diameter of 75% concentrates on 5 ~ 15 μm Between, lycopene carrying capacity is 34.87mg/g;Use ultrasonic wave added emulsifying can effectively facilitate microcapsule particle uniform concentration, it is to avoid Because the morphosis of lycopene microcapsule is destroyed by high shear, spray drying method is greatly improved lycopene microcapsule Dispersibility and dissolubility, improve the biological value of lycopene.
(6) secondary is used to be coated the preparation of lycopene microcapsule: micro-at above-mentioned steps (5) the most coated lycopene On the basis of capsule, use secondary coating technique that the microcapsule of the most coated lycopene is coated further and is improved, Secondary is coated the technique of the preparation of lycopene microcapsule and uses porous-starch consumption by 0.16%, and beta-schardinger dextrin-consumption is pressed 0.16%, adsorption temp 50 DEG C, adsorption time 30 min, the double coated lycopene microcapsule embedding rate prepared with this understanding Up to 97.75%, the double coated lycopene mean diameter prepared is 16.67 μm, and the Microcapsules Size scope of 80% is 10 ~ 24 μm, lycopene carrying capacity is 40.70 mg/g.
(7) freeze-day with constant temperature method prepares double coated lycopene microcapsule: be coated lycopene through above-mentioned steps (6) secondary micro- After capsule is adsorbed by porous-starch, it is dried in the thermostatic drying chamber of 50 DEG C, finally gives double coated lycopene microcapsule Product, advantageously in storage and the preservation of product.
In the present invention, once it is coated lycopene microcapsule and uses with arabic gum and modified starch for wall material, use super Lycopene is carried out microcapsule embedded by sound co-emulsifier and spray drying method.Examined by experiment of single factor and uniform design Examine different formulations and technological parameter, use orthogonal to optimize each factor, obtain embedding optimum process and be: arabic gum with Modified starch ratio 1:2(m/m), solid content 10%, core wall is than 1:1(m/m), tween 80 consumption 2%, at 30 DEG C, 160W bar Ultrasonic emulsification 15min under part, spray drying inlet temperature 190 DEG C, leaving air temp 80 DEG C, atomisation pressure 18MPa, microcapsule embedded Efficiency is up to 85.12%, and productivity is 60.50%;Lycopene carrying capacity is 34.87mg/g, and mean diameter is 8.13 μm, the grain of 75% Footpath concentrates between 5 ~ 15 μm.
In the present invention, although the most coated lycopene microcapsule has reached an ideal embedding effect, right Lycopene serves certain protective effect, but is found by Storage experiment, As time goes on, is once coated Fructus Lycopersici esculenti Red pigment microcapsule easily produces Electrostatic Absorption, the phenomenon of adhesion in bulk, it is contemplated that the hole adsorption on porous-starch surface, adopts With secondary coating technique, the microcapsule of the most coated lycopene it is coated further and improves, using double coated technology Have studied lycopene microcapsule preparation technology, once embed lycopene by ultrasonic emulsification and spray drying method, then with many Hole starch adsorption is once coated microcapsule, obtains double coated optimum preparation technology with experiment of single factor and response surface design optimization For: porous-starch consumption 0.16%(4 g), beta-schardinger dextrin-consumption 0.16%(4 g), adsorption temp 50 DEG C, adsorption time 30 min。
In the present invention, use secondary to be coated microcapsule technology and process lycopene, wherein utilize ultrasonic emulsification to carry out Fructus Lycopersici esculenti The first time of red pigment is coated, and improves the biological value of lycopene, after being coated through first time, then is coated material with starch based etc. Expect that forming second time by spray treatment is coated, and obtains that granule size is suitable, the suitable novel double coated lycopene of shape is micro- Capsule product, the lycopene microcapsule cis-isomer ratio of preparation is 45-50%, and bioavailability is high;Embedding rate up to 97.75%, lycopene carrying capacity is 40.70 mg/g, it is to avoid the loss of raw material and waste;Mean diameter is 16.67 μm, 80% Microcapsules Size scope in 10 ~ 24 μm, particle shape is uniform, and storage-stable is good;Room temperature keeps 3 months, tomato red Element can conservation rate more than 90%.
Following beneficial effect can be reached by the summary of the invention implementing the present invention concrete.
(1) present invention takes the lead in applying in the conversion of lycopene cis-trans-isomer superhigh pressure technique, passes through supertension Processing and the ratio of other conditional regulatory lycopene cis-trans-isomer and quantity, cis-isomer ratio is at 45-50%, biological Availability is high;Embedding rate is up to 97.75%, and lycopene carrying capacity is 40.70 mg/g, it is to avoid the loss of raw material and waste;Flat All particle diameters are 16.67 μm, and the Microcapsules Size scope of 80% is in 10 ~ 24 μm, and particle shape is uniform, and storage-stable is good; Room temperature keep 3 months, lycopene can conservation rate more than 90%, significantly improve Lycopene Function effect.
(2) lycopene produced at present is once coated microcapsule product, there is the biggest static behaviour and water absorption, easily Reunite, the quality problems such as caking, for solving problem above, the present invention uses double coated technology to prepare the micro-glue of lycopene Capsule, after not only making inclusion, water solublity and the stability of lycopene are greatly improved, and overcome the most coated common lycopene The quality problems that the granularity less (below 300 mesh) of microcapsule product causes, have huge static behaviour and water absorption, easily send out The quality problems such as raw reunion, caking so that coating rate reaches more than 90%, improves the skill of Xinjiang Tomatoes red pigment microcapsule product Art level.
Accompanying drawing explanation
Fig. 1 is shown with double coated method and prepares the process chart of lycopene microcapsule.
Fig. 2 is shown as the lycopene full wavelength scanner figure before ultra high pressure treatment.
Fig. 3 is shown as the lycopene full wavelength scanner figure after ultra high pressure treatment.
Fig. 4 is shown as the high-efficient liquid phase chromatogram of Pure Lycopene.
Fig. 5 is shown as the UV-Vis spectrogram of lycopene standard sample.
Fig. 6 is shown as the high-efficient liquid of lycopene and is separated chromatogram.
Fig. 7 is shown as the full wavelength scanner figure at HPLC chromatogram peak 1 after ultra high pressure treatment.
Fig. 8 is shown as the full wavelength scanner figure at HPLC chromatogram peak 2 after ultra high pressure treatment.
Fig. 9 is shown as the full wavelength scanner figure at HPLC chromatogram peak 3 after ultra high pressure treatment.
Figure 10 is shown as the full wavelength scanner figure at HPLC chromatogram peak 4 after ultra high pressure treatment.
Figure 11 is shown as the full wavelength scanner figure at HPLC chromatogram peak 5 after ultra high pressure treatment.
Porous-starch consumption (g) experimental result picture in Figure 12 double coated lycopene microcapsule single factor test.
Beta-schardinger dextrin-consumption (g) experimental result picture in Figure 13 double coated lycopene microcapsule single factor test.
Adsorption time (min) experimental result picture in Figure 14 double coated lycopene microcapsule single factor test.
Adsorption temp (DEG C) experimental result picture in Figure 15 double coated lycopene microcapsule single factor test.
Figure 16 is that in double coated lycopene microcapsule, adsorption temp responds with porous-starch consumption reciprocal effect embedding rate Face figure.
Figure 17 is that in double coated lycopene microcapsule, adsorption temp responds with beta-schardinger dextrin-consumption reciprocal effect embedding rate Face figure.
Figure 18 is that in double coated lycopene microcapsule, beta-schardinger dextrin-responds with porous-starch consumption reciprocal effect embedding rate Face figure.
Figure 19 is shown as once being coated the SEM photo of lycopene microcapsule.
Figure 20 is shown as the SEM photo of double coated lycopene microcapsule.
Figure 21 is shown as lycopene product release in vitro result comparison figure in simulated gastric fluid.
Figure 22 is shown as in simulated intestinal fluid without lycopene product release in vitro result comparison figure during cholate.
Lycopene product release in vitro result comparison figure when Figure 23 is shown as in simulated intestinal fluid adding cholate.
Detailed description of the invention
Below, for embodiment, the present invention is described, but, the present invention is not limited to following embodiment, basic in the present invention The % related to is percentage by weight meter without specializing.
Experiment supplementary material and reagent: Fructus Lycopersici esculenti is primary raw material;With porous-starch, beta-schardinger dextrin-, transmutability starch JX-001, Arabic gum is adjuvant;Pure Lycopene (lycopene purity 97%) is purchased from Shanghai to prestige Chemical Co., Ltd.;Normal hexane For analytical pure;Beijing sunlight Yi Cai Science and Technology Ltd.;Sodium alginate food stage, Qingdao Mingyue Marine Alga Group Corp., Ltd.;Bright Glue food stage, Ai Saer biotech inc, Xinjiang.
Key instrument and equipment: UHP900 × 2-Z ultra high pressure treatment device, it is public that high pressure science and technology Limited Liability is sent out by packet header section Department;V-2102PCS type ultraviolet-uisible spectrophotometer, UNICO(Shanghai) Instruments Co., Ltd.;High performance liquid chromatograph, Beijing Innovation Tong Heng Science and Technology Ltd.;Chromatographic column: YMC CarotenoidS-5 (4.6mm × 250mm);EYELA Spray Dryer SD-1000 Tokyo Rikakikai Co Ltd;KQ-400KDE type high power numerical control ultrasonic cleaner city of Kunshan Ultrasound Instrument Device company limited;RE-52A rotary evaporator Shanghai Yarong Biochemical Instrument Plant;PL203 electronic balance Mettler-Toledo Group;Medical Instruments factory of JJ-6 digital display DC constant speed stirrer Jintan City;V-1100D visible spectrophotometer Shanghai U.S. composes Reach Instrument Ltd.;79-2 Bidirectional magnetic agitator Community of Jin Tan County city Jin Cheng Guo Sheng experimental apparatus factory;DHG-9140A type electricity Hot constant temperature blast drying oven;The Motio AE31 micro-digital code camera of Nikon etc..
The all Fructus Lycopersici esculenti raw and auxiliary materials selected in the present invention, selected all reagent and instrument are all for it is well known that choosing , but it being not intended to the enforcement of the present invention, other reagent more well known in the art and equipment are applied both to below the present invention The enforcement of embodiment.
Embodiment one: the preparation of lycopene microcapsule
Referring to the drawings 1, the method using double coated method to prepare lycopene microcapsule, specifically comprise the following steps that
(1) preparation of tomato peel: select without going mouldy tomato peel, removes impurity removing, and with clear water by the earth on skin slag, Foreign material cleaned standby seam.
(2) lycopene oleo-resinous is prepared: the tomato peel of above-mentioned preparation is used supercritical CO2Extraction, pressure 28MPa, extraction temperature are at 70-72.5 DEG C, and CO flow 2500 2600kg/h, extraction time: 120min, in these process conditions Under, available purity reaches the lycopene of more than 90%;By by supercritical CO in tomato peel2The Fructus Lycopersici esculenti of 6% be obtained by extraction Red pigment oleoresin is as raw material, it is ensured that without any chemical composition and dissolvent residual on raw material, safety non-toxic.
(3) lycopene purifying process: use lycopene oleo-resinous above-mentioned steps (2) provided by 1:10(w/v) Solid-liquid ratio be dissolved in normal hexane, after magnetic agitation 10min, place room temperature cooling, place into-18 DEG C of refrigerator cooling stand 12h Rear sucking filtration obtains crystal of lycopene body, by after this step repeatedly purification three times lycopene, purity is 41.8% after measured.
(4) supertension isomerization processes, the lycopene of preparation cis ratio: purification mistake above-mentioned steps (3) prepared Lycopene oleo-resinous, be dissolved in, according to every 5mg lycopene oleo-resinous, the normal hexane that concentration is 50 g/mL, install to poly-second In alkene complex pocket, vacuum seals, at 500Mpa, and supertension 10min at 50 DEG C, finally give cis-isomer ratio 45.69%, contain Amount is the lycopene of 103.24mg/g, then uses high performance liquid chromatography to separate it, finally gives cis Fructus Lycopersici esculenti Red pigment;Use ultra high pressure treatment means effectively to promote lycopene to be changed into cis-structure from transconfiguration, Fructus Lycopersici esculenti will not be hydrolyzed Other effective ingredient in red pigment, moreover it is possible to play the effect of cold sterilization.
(5) employing is once coated the preparation of lycopene microcapsule: utilize ultrasonic emulsification and spray drying method to carry out Fructus Lycopersici esculenti The first time of red pigment is coated, with arabic gum and modified starch for wall material, and arabic gum and modified starch ratio 1:2(m/m), Gu Shape thing content 10%, core wall is than 1:1(m/m), tween 80 consumption 2%, at 30 DEG C, ultrasonic emulsification 15min under the conditions of 160W, spraying Being dried inlet temperature 190 DEG C, leaving air temp 80 DEG C, atomisation pressure 18MPa, microcapsule embedded efficiency is up to 85.12%, and productivity is 60.50%;The lycopene microcapsule mean diameter that is once coated obtained is 8.13 μm, and the particle diameter of 75% concentrates between 5 ~ 15 μm, Lycopene carrying capacity is 34.87mg/g;Use ultrasonic wave added emulsifying can effectively facilitate microcapsule particle uniform concentration, it is to avoid because of height The morphosis of lycopene microcapsule is destroyed by speed shearing force, and spray drying method is greatly improved dividing of lycopene microcapsule Dissipate property and dissolubility, improve the biological value of lycopene;
(6) secondary is used to be coated the preparation of lycopene microcapsule: although the most coated lycopene microcapsule reaches One ideal embedding effect, is served certain protective effect, but is found by Storage experiment lycopene, As time goes on, once it is coated lycopene microcapsule and easily produces Electrostatic Absorption, the phenomenon of adhesion in bulk, it is contemplated that be many The hole adsorption on starch surface, hole, uses secondary coating technique that the microcapsule of the most coated lycopene is entered one Step is coated and improves, and secondary is coated the technique of the preparation of lycopene microcapsule and uses porous-starch consumption 4 g, and beta-schardinger dextrin-is used Measure 4 g, adsorption temp 50 DEG C, adsorption time 30min, the double coated lycopene microcapsule embedding rate prepared with this understanding Up to 97.75%, the double coated lycopene mean diameter prepared is 16.67 μm, and the Microcapsules Size scope of 80% is 10 ~ 24 μm, lycopene carrying capacity is 40.70 mg/g.
(7) freeze-day with constant temperature method prepares double coated lycopene microcapsule: through secondary, above-mentioned steps is coated lycopene Microcapsule, after porous-starch adsorbs, is dried in the thermostatic drying chamber of 50 DEG C, finally gives double coated lycopene microcapsule Product, advantageously in storage and the preservation of product.
The lycopene microcapsule using above-mentioned double coated microcapsule technology to prepare, obtains that granule size is suitable, shape is closed Suitable novel double coated lycopene microcapsule product, the lycopene microcapsule cis-isomer ratio of preparation at 45-50%, Bioavailability is high;Embedding rate is up to 97.75%, and lycopene carrying capacity is 40.70 mg/g, it is to avoid the loss of raw material and wave Take;Mean diameter is 16.67 μm, and the Microcapsules Size scope of 80% is in 10 ~ 24 μm, and particle shape is uniform, storage-stable Well;Room temperature keeps 3 months, and lycopene can conservation rate more than 90%.
Embodiment two: use supertension to prepare All-cislycopene
By lycopene sample n-hexane dissolution, concentration is 50 g/mL, installs to vacuum in polyethylene complex pocket and seals. Different pressures, the time and at a temperature of carry out ultra high pressure treatment, investigate the internal isomerisation degree of lycopene and lycopene contain Amount.
The impact on lycopene isomerization of the different ultra-high pressure treatment conditions: by different pressures, the time and at a temperature of Carry out ultra high pressure treatment, investigate the internal isomerisation degree of lycopene and content of lycopene.The results are shown in Table 1.
Table 1: the different disposal condition impact on lycopene isomerization
Sample All-cislycopene ratio (%) Content of lycopene (mg/g)
Untreated samples 13.25% 52.37mg/g
400Mpa, 10min, 50 DEG C 34.76% 87.94mg/g
500Mpa, 10min, 50 DEG C 45.69% 103.24mg/g
500Mpa, 10min, room temperature 43.23% 98.79mg/g
500Mpa, 8min, 50 DEG C 39.51% 97.67mg/g
As shown in Table 1, after the ultra high pressure treatment of 500Mpa, 10min, 50 DEG C, lycopene either cis ratio is also It it is the sample after content all processes apparently higher than other conditions.
With ultraviolet-visible spectrophotometer, the lycopene sample liquid after ultra high pressure treatment is carried out UV-Vis spectrum to sweep Retouch, and compare with the UV-Vis spectral scan spectrogram of untreated lycopene sample liquid, by observing between the two Difference determine ultra high pressure treatment after lycopene sample liquid in whether there is cis-isomer, pass through ultraviolet-visible spectrum Identify the Lycopene structure in supertension lycopene sample.
The lycopene of alltrans can be identified by retention time and ultraviolet-visible spectrogram.Lycopene suitable Formula isomer can be identified by the wavelength nm number of each major absorbance peak of full wavelength scanner figure and Q-value.Q-value is i.e. Acis/Atrans。
UV-Vis(UV scanning) identify isomers of lycopene: by the lycopene sample before and after processing is carried out entirely Length scanning, before and after discovery processes, lycopene wavelength has significantly change, occurs in that document is reported in appearance at 362nm Cis peak.
Referring to the drawings 2 is the lycopene solution full wavelength scanner figure before ultra high pressure treatment, after accompanying drawing 3 is ultra high pressure treatment Lycopene solution full wavelength scanner figure, it is known that in two full wavelength scanner figures, lycopene is respectively at 447,471,503 nm There are 3 maximum absorption wavelengths at place, but the characteristic absorption spectrum of the lycopene in the lycopene liquid after ultra high pressure treatment is sent out Having given birth to change, occurred in that characteristic absorption peak near ultraviolet band 361 nm, the characteristic absorption of this wavelength is due to trans tomato red Element is isomerized to cis-isomer and causes, and therefore tentatively ultra high pressure treatment the structure of lycopene can be made to there occurs change Change.
Different structure body in HPLC isolation identification lycopene sample.
Chromatographic column: YMC CarotenoidS-5 (4.6mm × 250mm);Mobile phase A: containing acetonitrile, the methanol mixed of 0.05% Liquid (acetonitrile: methanol is 3:1);Mobile phase B: containing the MTBE solution of 0.05%, gradient elution;Mobile phase B: in 8min, 0 ~ 55% (V/ V);8 ~ 35min: maintain 55% (V/V);Flow velocity: 1mL/min.
Sample size is 20 μ L, and detection wavelength is 471nm, and component retention time and spectral signature according to isolated determine Cis-trans-isomer, the content of cis-trans-isomer in sample is determined by area normalization method.
Referring to the drawings 4, the component separated is carried out Preliminary Identification, from full wavelength scanner figure, referring to the drawings 5, draw above 5 Individual peak is same types of materials, it can be assumed that be the isomer of lycopene.Sample after contrast ultra high pressure treatment separates through HPLC The UV-Vis spectrum of 5 detached peakses of rear gained is visible, referring to the drawings 6 to accompanying drawing 11, except the sound of composition corresponding to Rt=33.607 Between Ying Shi consistent with all-trans lycopene, can substantially assert that it is all-trans lycopene, other four peak (Rt= 28.307,29.790,31.923,38.007) composition corresponding in UV-Vis spectrum in the peak type of 440-500nm wavelength section Similar to alltrans tomato red, but its peak position has the violet shift of 3-10nm, goes out useful stronger absworption peak at 361nm, with cis simultaneously The UV-Vis spectrum of structure lycopene is consistent.
Conclusion: under the conditions of the ultra high pressure treatment of 500Mpa, 10min, 50 DEG C, lycopene either cis ratio is still Content is all apparently higher than the sample after the process of other conditions.The cis-isomer ratio of lycopene is at 45-50%, lycopene Content is 103.24mg/g.The component separated is carried out Preliminary Identification, show that above 5 peaks are same type from full wavelength scanner figure Material, it can be assumed that be the isomer of lycopene.Further infer that to prove four kinds that wherein four kinds of compositions are lycopene suitable Formula isomer, can be separated and carry out next step use.
Embodiment three: lycopene microcapsule is once coated engineer testing
Determined by experiment of single factor and be once coated the selection of lycopene wall material, wall material component ratio, core wall ratio, emulsifying Agent consumption and solid content, use ultrasonic wave added emulsion process that the most coated lycopene microcapsule emulsion is carried out breast Change, utilizing to be spray-dried, it is dried.Owing to ultrasonic wave added emulsifying and spray drying relate to many kinds of parameters, select uniformly to set Each parameter is screened and significance analysis by meter experimental technique, finally determines that two affect in the most significant factor and single factor test Two factors the most significant use orthogonal experiment optimization together, thus obtain optimum process and formula.
Conclusion: ultrasonic wave added emulsifying and spray drying method are prepared lycopene microcapsule optimum process and be: arabic gum with Modified starch ratio is 1:2(m/m), solid content 10%, core wall is than 1:1(m/m), tween 80 consumption 2%, at 30 DEG C, 160W Under the conditions of ultrasonic emulsification 10min, be spray-dried inlet temperature 190 DEG C, leaving air temp 80 DEG C, atomisation pressure 18Mpa, microcapsule imitate Rate is up to 85.12%, and productivity is 60.50%, lycopene carrying capacity 34.87mg/g, and mean diameter is 8.13 μm, the particle diameter collection of 75% In between 5 ~ 15 μm.
Embodiment four: double coated prepare lycopene microcapsule experiment of single factor
1. lycopene microcapsule prepares experiment of single factor
Double coated prepare lycopene microcapsule during embedding rate influenced by factors, such as the use of porous-starch Amount, the consumption of beta-schardinger dextrin-, the adsorption time of porous-starch, and the adsorption temp etc. of porous-starch.
The 1.1 porous-starch consumptions impact on microcapsule effect: in the case of other conditions are certain, weigh and once wrap By lycopene microcapsule 1g, the content of porous-starch is respectively by 1 g, 2 g, 4 g, 6 g, 8 g;Prepare double coated by 1.2.2 Lycopene microcapsule, and calculate its On Technique of Microencapsulation of Lycopene embedding rate.
The consumption of the 1.2 beta-schardinger dextrin-s impact on microcapsule effect: take above-mentioned optimal result, weighs and is once coated Fructus Lycopersici esculenti Red pigment microcapsule 1 g, the content of porous-starch is 4 g, and the consumption of beta-schardinger dextrin-is respectively by 1 g, 2 g, 3 g, 4 g, 6 g, 8 g;Prepare double coated lycopene microcapsule by 1.2.2, and calculate its On Technique of Microencapsulation of Lycopene embedding rate.
The 1.3 porous-starch adsorption times impact on microcapsule effect: take above-mentioned optimum results, weighs and is once coated kind Lycopene microcapsule 1 g, the content of porous-starch is 4 g, and the consumption of beta-schardinger dextrin-is 4 g, and adsorption time is respectively 15 min, 30 min, 45 min, 60 min;Prepare double coated lycopene microcapsule by 1.2.2, and calculate its On Technique of Microencapsulation of Lycopene Embedding rate.
The 1.4 porous-starch adsorption temps impact on microcapsule effect: weigh and be once coated lycopene microcapsule 1 g, The content of porous-starch is 4 g, and the consumption of beta-schardinger dextrin-is 4 g, and the adsorption time of porous-starch is 30 min, porous-starch Adsorption temp presses 40 DEG C respectively, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C;It is prepared as described above double coated lycopene microcapsule, and Calculate its On Technique of Microencapsulation of Lycopene embedding rate.
Experiment of single factor result: 12 understanding referring to the drawings, porous-starch can promote the formation of microcapsule within the specific limits, But when its reach saturated after, the most no longer adsorb;And it can be observed from fig. 13 that beta-schardinger dextrin-is as wall material, mistake in emulsion Amount interpolation can extrude in type microcapsule, causes microcapsules rupture;The adsorption time of porous-starch also has certain limit value, as Figure 14, when after adsorption time to 30 min, continues over time, and micro encapsulation embedding rate gradually tends to saturation balance state;Figure 15 show that temperature is more apparent to embedding impact effect, make molecular motion velocities accelerate this is because temperature raises, expand between molecule Dissipating aggravation, promote lycopene to porous-starch diffusion inside, but temperature is too high that wall material character may can be caused again to change (as occurred starch gelatinization or starch structure to be destroyed), causes lycopene microcapsule embedding rate to decline.
In sum, porous-starch consumption 4 g, beta-schardinger dextrin-consumption 4 g, adsorption time 30 min, adsorption temp are chosen Double coated experiment of single factor best results when being 50 DEG C, converts the meter that is weight percentage, porous-starch consumption 0.16%, and β-ring is stuck with paste Essence consumption 0.16.
Embodiment five: the optimization experiment of the double coated technological parameter of lycopene microcapsule
On the basis of single factor test, use response phase method to porous-starch consumption, beta-schardinger dextrin-consumption, porous-starch absorption temperature Spending three factors to be optimized, with microcapsule embedded rate as index, quadrature factor water-glass is shown in Table 2.
Table 2: response phase method analysis factor and water-glass
Response phase method optimization experiment result: by practical operation and above-mentioned experiment of single factor analysis, finds adsorption time pair The impact of microcapsule embedded rate is inconspicuous, therefore casts out, and chooses porous-starch consumption, beta-schardinger dextrin-consumption, porous-starch adsorption temp Carry out the response surface analysis of Three factors-levels, with the embedding rate of double coated microcapsule as response value, the results are shown in Table: 3.
Table 3: response surface optimization EXPERIMENTAL DESIGN and result
Standard sequence Run sequence Porous-starch consumption/g (X1) Beta-schardinger dextrin-consumption/g (X2) Adsorption temp/DEG C (X3) Embedding rate/%
11 1 0 -1 1 93.01%
4 2 1 1 0 91.13%
8 3 1 0 1 90.84%
12 4 0 1 1 95.96%
13 5 0 0 0 97.75%
15 6 0 0 0 96.76%
9 7 0 -1 -1 97.05%
10 8 0 1 -1 91.07%
3 9 -1 1 0 94.82%
2 10 1 -1 0 96.09%
6 11 1 0 -1 94.53%
1 12 -1 -1 0 97.23%
14 13 0 0 0 96.31%
7 14 -1 0 1 96.75%
5 15 -1 0 -1 94.78%
Table 4: regression model coefficient and significance test result
? Coefficient Factor standard is by mistake T P Significance
Constant 0.969400 0.005469 177.252 0.000
X1 -0.013737 0.003349 -4.102 0.009 **
X2 -0.013000 0.003349 -3.882 0.012 *
X3 -0.001087 0.003349 -0.325 0.759
X1*X1 -0.010850 0.004930 -2.201 0.079
X2*X2 -0.010375 0.004930 -2.105 0.089
X3*X3 -0.016300 0.004930 -3.306 0.021 *
X1*X2 -0.006375 0.004736 -1.346 0.236
X1*X3 -0.014150 0.004736 -2.988 0.031 *
X2*X3 0.022325 0.004736 4.714 0.005 **
Table 5: the significance test of regression model
Source Degree of freedom Seq SS Adj SS Adj MS F P Significance
Return 9 0.007417 0.007417 0.000824 9.18 0.013 *
Linearly 3 0.002871 0.002871 0.000957 10.67 0.013 *
Square 3 0.001589 0.001589 0.000530 5.90 0.043
Reciprocal action 3 0.002957 0.002957 0.000986 10.98 0.012 *
Residual error error 5 0.000449 0.000449 0.000090
Lose and intend 3 0.000340 0.000340 0.000113 2.09 0.340
Pure error 2 0.000109 0.000109 0.000054
Add up to 14 0.007866
Note: * is notable (p < 0.05);* is extremely notable (p < 0.01).
Experiment is carried out with random order, using microcapsule embedded rate as response value, uses Minitab15.0 data statistics to divide Analysis software carries out multiple regression matching to test data, and regression model coefficient and significance test the results are shown in Table 3.Obtain matching to return The equation is returned to be:
Y(%)
=0.969400-0.013737X1-0.013000X2-0.001087X3-0.010850X1X1-0.010375X2X2- 0.016300X3X3-0.006375X1X2-0.014150X1X3+0.022325X2X3。
First order X1 is extremely notable as shown in Table 3, illustrates that the consumption of porous-starch is the most notable to embedding rate;X2 is notable;Double items X3*X3 is notable;Mutual item X2*X3 is extremely notable, and X1*X3 is notable, illustrates that the change of response value is considerably complicated, each factor pair of test The impact of lycopene microcapsule envelop rate is not simple linear relationship.Found out by table 4 analysis result, F=9.18 > F0.05 (9,9)=3.18, p < 0.05, show that regression model is notable.Linear mistake intends item F=2.09 < F0.05 (9,3)=8.81, p=0.340 > 0.05, significantly, illustrates that this models fitting degree is good, and test error is little, can be as forecast model.Embedding rate is affected Factor size is followed successively by: porous-starch consumption, beta-schardinger dextrin-consumption, adsorption temp.
By three-dimensional response diagram, see accompanying drawing 16-18 and can intuitively reflect the reciprocal action of each factor of this model And the impact on response value.In conjunction with practical operation and confirmatory experiment, carry out three times and repeat, draw the double-contracting under this optimal conditions By microcapsule embedded rate up to 97.75%, illustrate that this model prediction is good, can be as model prediction optimal procedure parameters, Excellent microcapsule preparation process is: porous-starch consumption 4 g, beta-schardinger dextrin-consumption 4 g, adsorption temp 50 DEG C, adsorption time 30 Min, the double coated lycopene microcapsule embedding rate prepared with this understanding up to 97.75%, lycopene carrying capacity 40.70 mg/g。
Conclusion: double coated optimum preparation technology is: porous-starch consumption 4 g(0.16%), beta-schardinger dextrin-consumption 4 g (0.16%), adsorption temp 50 DEG C, adsorption time 30 min, double coated lycopene microcapsule embedding rate up to 97.75%, kind Lycopene carrying capacity 40.70 mg/g.
Embodiment six: the effective evaluation of double coated On Technique of Microencapsulation of Lycopene technical specification
Accurately weigh double coated microcapsule product and put in color comparison tube, add normal hexane, after constant speed concussion certain time, very Empty sucking filtration, and with the lycopene of normal hexane washing surface of microcapsule residual to filtrate to colourless.After sucking filtration, microcapsule produces Product are positioned in 50 DEG C of thermostatic drying chambers and are dried 30 min, weigh, and calculate double coated microcapsule embedded rate by formula.
M1: microcapsule product (g)
M2: filter paper quality (g)
M3: microcapsule and filter paper gross mass (g) after drying
Lycopene carrying capacity calculates
C: lycopene solution concentration (μ g/mL)
V: lycopene solution volume (mL)
M: lycopene microcapsule quality (g)
1.2.3 lycopene maximum absorption wavelength determines that taking a small amount of lycopene crystal is dissolved in normal hexane, uses ultraviolet Spectrophotometer is at 300 ~ 600nm range scans.
1.2.4 the drafting lycopene standard solution of lycopene standard curve: accurate weighing Pure Lycopene 2.5mg, dissolves with 5mL dichloromethane, is transferred in 50mL brown volumetric flask, utilizes ultrasound wave dissolution.Fixed with normal hexane Hold to 50mL, be configured to the storing solution of 50 μ g/mL.
The drafting of standard working curve: the most accurately pipette 0.1,0.2,0.3,0.4,0.5,0.6,0.7,0.8,0.9, 1.0mL lycopene standard solution is placed in 10mL brown volumetric flask, uses normal hexane constant volume, uses ultraviolet spectrometry light under 471nm Degree meter colorimetric.
Scanning electron microscope SEM observation structure:
Solid sample particles is distributed on silicon chip, uses vacuum sputtering instrument metal spraying 5min under vacuum conditions, then clap According to.
Conclusion:
(1) double coated optimum preparation technology is: porous-starch consumption 4 g(0.16%), beta-schardinger dextrin-consumption 4 g (0.16%), adsorption temp 50 DEG C, adsorption time 30 min, double coated lycopene microcapsule embedding rate up to 97.75%, kind Lycopene carrying capacity 40.70 mg/g.
(2) referring to the drawings 19 and 20, once it is coated the microcapsule granule size of gained the most all in 5-10 μ m, for Surface has the granule of rough approximate spheres, this situation can reduce the compactness of cyst wall, causes productivity and the effect of product Rate has declined;Double-deck coated microcapsule becomes bigger grain shape, and granular size is in 10-20 μ m.Due to secondary It is coated the absorbability that wall material porous-starch is stronger, is effectively increased the embedding rate of double coated lycopene microcapsule.
Embodiment seven: the release in vitro rate experiment of lycopene product
By the outer gastrointestinal environment of analogue body, investigate lycopene oleo-resinous, lycopene and be once coated microcapsule, tomato red Element secondary is coated the release in vitro effect of microcapsule and commercially available soft capsule of lycopene.Wherein, simulated gastric fluid is pH2.0 Hydrochloric acid solution add pepsin 0.32g/100mL.When measuring the release rate in simulated intestinal fluid, point two groups of comparisons, examine simultaneously Examine the cholate impact on 4 series products release rates.Two groups of simulated intestinal fluid formula are respectively as follows: the potassium dihydrogen phosphate of (1) pH7.2 (containing 0.5g/100mL tween 80) adds trypsin 1g/100mL;(2) potassium dihydrogen phosphate of pH7.2 is (containing 0.5g/ 100mL tween 80 and 1.5g/L cholate) add trypsin 1g/100mL.
The mensuration of lycopene release rate and calculating: the double coated lycopene microcapsule of accurate measuring lycopene, once It is coated each 1mL of microcapsule, soft capsule of lycopene and lycopene oleo-resinous, often group 3 parts, is respectively placed in tool plug test tube, often Individual test tube is separately added into release medium 50mL, sealing of jumping a queue.Each test tube is placed in Desk type constant-temperatureoscillator oscillator, (37.5 ± 0.5), under the conditions of DEG C, vibrate with 100r/min rpm level.Respectively at different time points (sample-adding vibration after 0.5,1,2,4,6,8, 10,12,15,18,21,24h) sampling 5mL, and supplement the fresh dissolution medium of same volume simultaneously.Taken sample 14000r/ Min is centrifuged 10min, takes supernatant and measures the content of lycopene, calculates accumulative release rate.
Conclusion: see accompanying drawing 21 to accompanying drawing 23, contrasts double coated lycopene microcapsule, is once coated the micro-glue of lycopene Lycopene product in capsule, lycopene oleo-resinous and commercially available soft capsule of lycopene 4, finds double coated lycopene microcapsule There is in simulated intestinal fluid more preferable slow-releasing, and release is the most thorough.Compared with commercially available soft capsule of lycopene, double coated kind Lycopene microcapsule be once coated lycopene microcapsule and have faster rate of release, compared with lycopene oleo-resinous, Double coated lycopene microcapsule all can preferably improve the biology of raising lycopene with being once coated lycopene microcapsule Utilization rate.
Above-described embodiment is only for clearly demonstrating example of the present invention, and not restriction to embodiment. For those of ordinary skill in the field, the change of other multi-form can also be made on the basis of the above description Or variation.Here without also cannot all of embodiment be given exhaustive.And the obvious change thus amplified out Or change among still in protection scope of the present invention.

Claims (1)

1. one kind uses lycopene microcapsule prepared by double coated method, it is characterised in that in percentage by weight, Fructus Lycopersici esculenti Prepared by the double coated method of red pigment microcapsule employing specifically comprises the following steps that
(1) preparation of tomato peel: select, without going mouldy tomato peel, to remove impurity removing, and with clear water by the earth on skin slag, foreign material Cleaned standby seam;
(2) lycopene oleo-resinous is prepared: the tomato peel of above-mentioned preparation is used supercritical CO2Extraction, pressure 28MPa, extraction Temperature at 70-72.5 DEG C, CO flow 2500 2600kg/h, extraction time 120min, under these process conditions, available pure Degree reaches the lycopene of more than 90%;By supercritical CO in tomato peel2The lycopene oleo-resinous of 6% be obtained by extraction is made For raw material in next step;
(3) lycopene purifying process: use lycopene oleo-resinous above-mentioned steps (2) provided by the feed liquid of 1:10w/v Ratio is dissolved in normal hexane, after magnetic agitation 10min, places room temperature cooling, places into the cooling of-18 DEG C of refrigerator and stands sucking filtration after 12h Crystal of lycopene body, by after this step repeatedly purification three times lycopene, purity is 41.8% after measured;
(4) supertension isomerization process, preparation cis ratio lycopene: purification prepared by above-mentioned steps (3) is crossed kind Lycopene oleoresin, is dissolved in the normal hexane of 100mL according to every 5mg lycopene oleo-resinous, installs in polyethylene complex pocket true Empty sealing, uses common extra-high tension unit, at 500Mpa, obtains cis-isomer ratio at 50 DEG C under the conditions of supertension 10min 45.69%, content is the lycopene of 103.24mg/g, then uses high performance liquid chromatography to separate it, finally gives suitable The lycopene of formula;
(5) employing is once coated the preparation of lycopene microcapsule: utilize ultrasonic emulsification and spray drying method to carry out lycopene First time be coated, with arabic gum and modified starch for wall material, arabic gum and modified starch ratio 1:2 based on m/m, solid Thing content 10%, core wall than 1:1, tween 80 consumption 2%, at 30 DEG C, ultrasonic emulsification 15min under the conditions of 160W, be spray-dried air intake Temperature 190 DEG C, leaving air temp 80 DEG C, atomisation pressure 18MPa, microcapsule embedded efficiency reaches 85.12%, and productivity is 60.50%;? To the lycopene microcapsule mean diameter that is once coated be 8.13 μm, the particle diameter of 75% concentrates between 5 ~ 15 μm, lycopene carry Amount is 34.87mg/g;
(6) secondary is used to be coated the preparation of lycopene microcapsule: at above-mentioned steps (5) the most coated lycopene microcapsule On the basis of, use secondary coating technique that the microcapsule of the most coated lycopene is coated further and is improved, secondary The technique of the preparation being coated lycopene microcapsule uses porous-starch consumption by 0.16%, and beta-schardinger dextrin-consumption presses 0.16%, inhales Enclosure temperature 50 DEG C, adsorption time 30 min, the double coated lycopene microcapsule embedding rate prepared with this understanding reaches 97.75%, prepare double coated lycopene mean diameter be 16.67 μm, the Microcapsules Size scope of 80% in 10 ~ 24 μm, Lycopene carrying capacity is 40.70 mg/g;
(7) freeze-day with constant temperature method prepares double coated lycopene microcapsule: be coated lycopene microcapsule through above-mentioned steps (6) secondary After being adsorbed by porous-starch, it is dried in the thermostatic drying chamber of 50 DEG C and prepares double coated lycopene microcapsule.
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